CN108854966A - A kind of preparation method of silica gel supported composite adsorbing material - Google Patents
A kind of preparation method of silica gel supported composite adsorbing material Download PDFInfo
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- CN108854966A CN108854966A CN201810804604.XA CN201810804604A CN108854966A CN 108854966 A CN108854966 A CN 108854966A CN 201810804604 A CN201810804604 A CN 201810804604A CN 108854966 A CN108854966 A CN 108854966A
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- carbon fiber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/024—Compounds of Zn, Cd, Hg
- B01J20/0244—Compounds of Zn
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0296—Nitrates of compounds other than those provided for in B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation methods of silica gel supported composite adsorbing material, including：(1) a certain amount of carbon fiber is added in deionized water, 2~5h of ultrasonic disperse obtains carbon fiber suspension, wherein contain 1~5g carbon fiber in 1L deionized water；(2) above-mentioned carbon fiber suspension is added in the zinc nitrate solution that mass concentration is 10%, is stirred evenly, it is 2~6 that acid solution, which is added, and adjusts the pH value of solution, obtains carbon fiber-zinc nitrate mixed solution；(3) under 50~60 DEG C of water bath conditions, a certain amount of above-mentioned carbon fiber-zinc nitrate mixed solution is added dropwise in silica solution, 3~4h of magnetic agitation, above-mentioned mixed sols is placed in 110~120 DEG C of dry 1~2h later, it is cooled to room temperature in drying box, obtains silica gel supported composite adsorbing material.Silica gel supported composite adsorbing material preparation process in the present invention is simple, at low cost, has preferable absorption property to heavy metal ion, and the chemical stability in acid medium is high.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation side of silica gel supported composite adsorbing material
Method.
Background technique
Heavy metal is generally widely present in nature with natural concentration.However, in recent decades, with modern industry
Development, the mankind are increasing to the exploitation of heavy metal, smelting, processing and business manufacturing activities, cause many heavy metals to enter big
Gas and water, soil environment cause serious environmental pollution.Therefore there can be the material for efficiently separating function to solution heavy metal ion
The exploitation of material be not only be resource circulation utilization effective means, and be the urgent needs of environmental pollution improvement.Administering method
It is concentrated mainly on microorganism remediation and chemical remediation.But the sediment containing heavy metal ion that these methods generate when administering is not
Stablize, be easy to cause secondary pollution, therefore develop the huge sum of money that preparation process is simple, low in cost, effect is obvious, without secondary pollution
Belong to ion adsorbent to be of great significance and broad prospect of application, be one section of period environmental technology field research from now on emphasis it
One.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of silica gel supported composite adsorbing material, energy
Enough solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of silica gel supported composite adsorbing material, to overcome existing skill
Deficiency in art.
To achieve the above object, the present invention provides the following technical solutions：
A kind of preparation method of silica gel supported composite adsorbing material, including：
(1) a certain amount of carbon fiber being added in deionized water, 2~5h of ultrasonic disperse obtains carbon fiber suspension,
In, 1~5g carbon fiber is contained in 1L deionized water；
(2) above-mentioned carbon fiber suspension is added in the zinc nitrate solution that mass concentration is 10%, is stirred evenly, acid is added
The pH value that liquid adjusts solution is 2~6, obtains carbon fiber-zinc nitrate mixed solution；
(3) under 50~60 DEG C of water bath conditions, by a certain amount of above-mentioned carbon fiber-, that zinc nitrate mixed solution is added dropwise to silicon is molten
In glue, above-mentioned mixed sols is placed in 110~120 DEG C of dry 1~2h later by 3~4h of magnetic agitation, cooling in drying box
To room temperature, silica gel supported composite adsorbing material is obtained.
Preferably, in step (1), 2~3g carbon fiber is contained in 1L deionized water.
Preferably, in step (2), the ratio between volume of the carbon fiber suspension and the zinc nitrate solution is 1:2~4.
Preferably, the ratio between volume of the carbon fiber suspension and the zinc nitrate solution is 1:3.
Preferably, in step (2), the acid solution uses hydrochloric acid solution.
Preferably, in step (3), the ratio between volume of the carbon fiber-zinc nitrate mixed solution and the silica solution is 1:3
~5.
Preferably, in step (3), the preparation method of the silica solution includes：
1) auxiliary agent potassium dihydrogen phosphate is added in the sulfuric acid solution that mass percent concentration is 22%, wherein biphosphate
The proportion of potassium and sulfuric acid solution is 0.5~1:100, obtain mixed liquor A；
2) auxiliary agent hexamethyldisiloxane is added in sodium silicate solution, wherein hexamethyldisiloxane and sodium silicate solution
Proportion be 0.5~1:100, obtain mixed liquid B；
3) mixed liquor A and mixed liquid B are mixed, is granulated into gel particles through synthetic reaction, then gel particles are placed in always
Change in pond, add aging agent aging, sour processing is carried out to gel particles using sour modifying agent, washing, drying, crushing and classification obtain
Silica solution.
Compared with the prior art, the advantages of the present invention are as follows：Silica gel supported composite adsorbing material preparation in the present invention
It is simple process, at low cost, there is preferable absorption property, and the chemical stability in acid medium to heavy metal ion
It is high.
Specific embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of silica gel supported composite adsorbing material, including：
(1) a certain amount of carbon fiber being added in deionized water, 2~5h of ultrasonic disperse obtains carbon fiber suspension,
In, 1~5g carbon fiber is contained in 1L deionized water；
(2) above-mentioned carbon fiber suspension is added in the zinc nitrate solution that mass concentration is 10%, is stirred evenly, acid is added
The pH value that liquid adjusts solution is 2~6, obtains carbon fiber-zinc nitrate mixed solution；
(3) under 50~60 DEG C of water bath conditions, by a certain amount of above-mentioned carbon fiber-, that zinc nitrate mixed solution is added dropwise to silicon is molten
In glue, above-mentioned mixed sols is placed in 110~120 DEG C of dry 1~2h later by 3~4h of magnetic agitation, cooling in drying box
To room temperature, silica gel supported composite adsorbing material is obtained.
In above-mentioned steps (1), 2~3g carbon fiber is contained in 1L deionized water.
In above-mentioned steps (2), the ratio between volume of the carbon fiber suspension and the zinc nitrate solution is 1:2~4, preferably
, the ratio between volume of the carbon fiber suspension and the zinc nitrate solution is 1:3；The acid solution uses hydrochloric acid solution.
In above-mentioned steps (3), the ratio between volume of the carbon fiber-zinc nitrate mixed solution and the silica solution is 1:3~
5, it is preferred that the ratio between volume of the carbon fiber-zinc nitrate mixed solution and the silica solution is 1:4.
In one embodiment, the preparation method of the silica solution includes：
1) auxiliary agent potassium dihydrogen phosphate is added in the sulfuric acid solution that mass percent concentration is 22%, wherein biphosphate
The proportion of potassium and sulfuric acid solution is 0.5~1:100, obtain mixed liquor A；
2) auxiliary agent hexamethyldisiloxane is added in sodium silicate solution, wherein hexamethyldisiloxane and sodium silicate solution
Proportion be 0.5~1:100, obtain mixed liquid B；
3) mixed liquor A and mixed liquid B are mixed, is granulated into gel particles through synthetic reaction, then gel particles are placed in always
Change in pond, add aging agent aging, sour processing is carried out to gel particles using sour modifying agent, washing, drying, crushing and classification obtain
Silica solution.
Following preparation methods that silica gel supported composite adsorbing material in the present invention is illustrated with specifically embodiment.
Embodiment 1
(1) a certain amount of carbon fiber is added in deionized water, ultrasonic disperse 2h obtains carbon fiber suspension, wherein 1L
Contain 1g carbon fiber in deionized water；
(2) 2 volumes, mass concentration is added in the above-mentioned carbon fiber suspension of 1 volume to stir in 10% zinc nitrate solution
It mixes uniformly, it is 2 that acid solution, which is added, and adjusts the pH value of solution, obtains carbon fiber-zinc nitrate mixed solution；
(3) under 50 DEG C of water bath conditions, carbon fiber-zinc nitrate mixed solution of 1 volume is added dropwise to the silica solution of 3 volumes
In, above-mentioned mixed sols is placed in 110 DEG C of dry 1h later, is cooled to room temperature in drying box, obtains silicon by magnetic agitation 3h
Glue support type composite adsorbing material.
Embodiment 2
(1) a certain amount of carbon fiber is added in deionized water, ultrasonic disperse 3h obtains carbon fiber suspension, wherein 1L
Contain 3g carbon fiber in deionized water；
(2) 3 volumes, mass concentration is added in the above-mentioned carbon fiber suspension of 1 volume to stir in 10% zinc nitrate solution
It mixes uniformly, it is 4 that acid solution, which is added, and adjusts the pH value of solution, obtains carbon fiber-zinc nitrate mixed solution；
(3) under 55 DEG C of water bath conditions, carbon fiber-zinc nitrate mixed solution of 1 volume is added dropwise to the silica solution of 4 volumes
In, above-mentioned mixed sols is placed in 115 DEG C of dry 1.5h later, is cooled to room temperature, obtains in drying box by magnetic agitation 3.5h
To silica gel supported composite adsorbing material.
Embodiment 3
(1) a certain amount of carbon fiber is added in deionized water, ultrasonic disperse 5h obtains carbon fiber suspension, wherein 1L
Contain 5g carbon fiber in deionized water；
(2) 4 volumes, mass concentration is added in the above-mentioned carbon fiber suspension of 1 volume to stir in 10% zinc nitrate solution
It mixes uniformly, it is 6 that acid solution, which is added, and adjusts the pH value of solution, obtains carbon fiber-zinc nitrate mixed solution；
(3) under 60 DEG C of water bath conditions, carbon fiber-zinc nitrate mixed solution of 1 volume is added dropwise to the silica solution of 5 volumes
In, above-mentioned mixed sols is placed in 120 DEG C of dry 2h later, is cooled to room temperature in drying box, obtains silicon by magnetic agitation 4h
Glue support type composite adsorbing material.
Silica gel supported composite adsorbing material preparation process in the present invention is simple, at low cost, has to heavy metal ion
Preferable absorption property, adsorption rate is up to 92.5~98.6%, and the chemical stability in acid medium is high.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (7)
1. a kind of preparation method of silica gel supported composite adsorbing material, which is characterized in that including：
(1) a certain amount of carbon fiber is added in deionized water, 2~5h of ultrasonic disperse obtains carbon fiber suspension, wherein 1L
Contain 1~5g carbon fiber in deionized water；
(2) above-mentioned carbon fiber suspension is added in the zinc nitrate solution that mass concentration is 10%, is stirred evenly, acid solution tune is added
The pH value for saving solution is 2~6, obtains carbon fiber-zinc nitrate mixed solution；
(3) under 50~60 DEG C of water bath conditions, a certain amount of above-mentioned carbon fiber-zinc nitrate mixed solution is added dropwise to silica solution
In, above-mentioned mixed sols is placed in 110~120 DEG C of dry 1~2h later, is cooled in drying box by 3~4h of magnetic agitation
Room temperature obtains silica gel supported composite adsorbing material.
2. the preparation method of silica gel supported composite adsorbing material according to claim 1, which is characterized in that step (1)
In, 2~3g carbon fiber is contained in 1L deionized water.
3. the preparation method of silica gel supported composite adsorbing material according to claim 1, which is characterized in that step (2)
In, the ratio between volume of the carbon fiber suspension and the zinc nitrate solution is 1:2~4.
4. the preparation method of silica gel supported composite adsorbing material according to claim 3, which is characterized in that the carbon fiber
Tieing up the ratio between volume of suspension and the zinc nitrate solution is 1:3.
5. the preparation method of silica gel supported composite adsorbing material according to claim 1, which is characterized in that step (2)
In, the acid solution uses hydrochloric acid solution.
6. the preparation method of silica gel supported composite adsorbing material according to claim 1, which is characterized in that step (3)
In, the ratio between volume of the carbon fiber-zinc nitrate mixed solution and the silica solution is 1:3~5.
7. the preparation method of silica gel supported composite adsorbing material according to claim 1, which is characterized in that step (3)
In, the preparation method of the silica solution includes：
1) mass percent concentration be 22% sulfuric acid solution in be added auxiliary agent potassium dihydrogen phosphate, wherein potassium dihydrogen phosphate with
The proportion of sulfuric acid solution is 0.5~1:100, obtain mixed liquor A；
2) auxiliary agent hexamethyldisiloxane is added in sodium silicate solution, wherein hexamethyldisiloxane and sodium silicate solution are matched
Than being 0.5~1:100, obtain mixed liquid B；
3) mixed liquor A and mixed liquid B are mixed, is granulated into gel particles through synthetic reaction, then gel particles are placed in aging pond
In, aging agent aging is added, sour processing is carried out to gel particles using sour modifying agent, it is molten to obtain silicon for washing, drying, crushing and classification
Glue.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905778A (en) * | 2020-08-24 | 2020-11-10 | 浙江工业大学台州研究院 | Supported catalyst, preparation method thereof and application thereof in synthesis of ethylbenzyl chloride |
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| CN101638218A (en) * | 2009-08-19 | 2010-02-03 | 中国科学院化学研究所 | Nano composite material, preparation method and application thereof |
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| US20160256851A1 (en) * | 2011-07-25 | 2016-09-08 | Leidos, Inc. | Reactive Self-Indicating Absorbent Materials, Methods, and Systems |
| CN107790103A (en) * | 2016-08-29 | 2018-03-13 | 中国石油化工股份有限公司 | A kind of composite adsorbing material and preparation method thereof |
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2018
- 2018-07-20 CN CN201810804604.XA patent/CN108854966A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566513A (en) * | 2003-06-27 | 2005-01-19 | 王家君 | Antibacterial active carbon fiber |
| CN101638218A (en) * | 2009-08-19 | 2010-02-03 | 中国科学院化学研究所 | Nano composite material, preparation method and application thereof |
| US20160256851A1 (en) * | 2011-07-25 | 2016-09-08 | Leidos, Inc. | Reactive Self-Indicating Absorbent Materials, Methods, and Systems |
| CN105289484A (en) * | 2015-04-02 | 2016-02-03 | 江苏沥泽生化科技有限公司 | Efficient adsorption activated carbon fiber cloth and preparation method thereof |
| CN107790103A (en) * | 2016-08-29 | 2018-03-13 | 中国石油化工股份有限公司 | A kind of composite adsorbing material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905778A (en) * | 2020-08-24 | 2020-11-10 | 浙江工业大学台州研究院 | Supported catalyst, preparation method thereof and application thereof in synthesis of ethylbenzyl chloride |
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